CN108239395A - A kind of lightweight reinforced polyamide composition and preparation method thereof - Google Patents
A kind of lightweight reinforced polyamide composition and preparation method thereof Download PDFInfo
- Publication number
- CN108239395A CN108239395A CN201611228126.XA CN201611228126A CN108239395A CN 108239395 A CN108239395 A CN 108239395A CN 201611228126 A CN201611228126 A CN 201611228126A CN 108239395 A CN108239395 A CN 108239395A
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- Prior art keywords
- polyamide
- acid
- inorganic powder
- hollow inorganic
- preferred
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- 229920002647 polyamide Polymers 0.000 title claims abstract description 106
- 239000004952 Polyamide Substances 0.000 title claims abstract description 104
- 239000000203 mixture Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 57
- 239000003365 glass fiber Substances 0.000 claims abstract description 40
- 239000004067 bulking agent Substances 0.000 claims abstract description 35
- 239000000463 material Substances 0.000 claims abstract description 23
- 229920003656 Daiamid® Polymers 0.000 claims abstract description 18
- 229920006141 Polyamide 5X Polymers 0.000 claims abstract description 16
- 229920005989 resin Polymers 0.000 claims abstract description 7
- 239000011347 resin Substances 0.000 claims abstract description 7
- 239000004615 ingredient Substances 0.000 claims abstract description 5
- 229920006122 polyamide resin Polymers 0.000 claims abstract description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 34
- 239000007822 coupling agent Substances 0.000 claims description 27
- 239000011521 glass Substances 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- -1 carbon dicarboxylic acids Chemical class 0.000 claims description 14
- 239000012752 auxiliary agent Substances 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 12
- 238000012986 modification Methods 0.000 claims description 11
- 230000004048 modification Effects 0.000 claims description 11
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 10
- 229910052799 carbon Inorganic materials 0.000 claims description 9
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 8
- 229920001577 copolymer Polymers 0.000 claims description 8
- 239000000178 monomer Substances 0.000 claims description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical class [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 6
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229920000305 Nylon 6,10 Polymers 0.000 claims description 5
- 238000005516 engineering process Methods 0.000 claims description 5
- 238000001125 extrusion Methods 0.000 claims description 5
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 4
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000001361 adipic acid Substances 0.000 claims description 4
- 235000011037 adipic acid Nutrition 0.000 claims description 4
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical class NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- BDJRBEYXGGNYIS-UHFFFAOYSA-N nonanedioic acid Chemical compound OC(=O)CCCCCCCC(O)=O BDJRBEYXGGNYIS-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 4
- BGHCVCJVXZWKCC-UHFFFAOYSA-N tetradecane Chemical compound CCCCCCCCCCCCCC BGHCVCJVXZWKCC-UHFFFAOYSA-N 0.000 claims description 4
- 229920006152 PA1010 Polymers 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 238000013019 agitation Methods 0.000 claims description 3
- 239000003963 antioxidant agent Substances 0.000 claims description 3
- 230000003078 antioxidant effect Effects 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000000805 composite resin Substances 0.000 claims description 3
- 150000001991 dicarboxylic acids Chemical class 0.000 claims description 3
- 239000000314 lubricant Substances 0.000 claims description 3
- 239000011976 maleic acid Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 239000002667 nucleating agent Substances 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 3
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 2
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 2
- 239000002028 Biomass Substances 0.000 claims description 2
- 229920002943 EPDM rubber Polymers 0.000 claims description 2
- 229920000571 Nylon 11 Polymers 0.000 claims description 2
- 229920000299 Nylon 12 Polymers 0.000 claims description 2
- 229920002292 Nylon 6 Polymers 0.000 claims description 2
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N Succinic acid Natural products OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 2
- KOEFSMLBFZGZLD-UHFFFAOYSA-L [bis(2-ethylhexoxy)-oxidophosphaniumyl] dihydrogen phosphate [bis(2-ethylhexoxy)-oxidophosphaniumyl] phosphate ethane-1,2-diolate titanium(4+) Chemical compound [Ti+4].[O-]CC[O-].CCCCC(CC)CO[P+]([O-])(OCC(CC)CCCC)OP(O)(O)=O.CCCCC(CC)CO[P+]([O-])(OCC(CC)CCCC)OP([O-])([O-])=O KOEFSMLBFZGZLD-UHFFFAOYSA-L 0.000 claims description 2
- 125000004423 acyloxy group Chemical group 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 2
- KDYFGRWQOYBRFD-NUQCWPJISA-N butanedioic acid Chemical compound O[14C](=O)CC[14C](O)=O KDYFGRWQOYBRFD-NUQCWPJISA-N 0.000 claims description 2
- QYMGIIIPAFAFRX-UHFFFAOYSA-N butyl prop-2-enoate;ethene Chemical compound C=C.CCCCOC(=O)C=C QYMGIIIPAFAFRX-UHFFFAOYSA-N 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 claims description 2
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- HDERJYVLTPVNRI-UHFFFAOYSA-N ethene;ethenyl acetate Chemical compound C=C.CC(=O)OC=C HDERJYVLTPVNRI-UHFFFAOYSA-N 0.000 claims description 2
- XPNLOZNCOBKRNJ-UHFFFAOYSA-N ethyl prop-2-enoate;methyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C=C.COC(=O)C(C)=C XPNLOZNCOBKRNJ-UHFFFAOYSA-N 0.000 claims description 2
- 229920006226 ethylene-acrylic acid Polymers 0.000 claims description 2
- 229920006245 ethylene-butyl acrylate Polymers 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 229920001912 maleic anhydride grafted polyethylene Polymers 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N phosphoric acid Substances OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 2
- 238000006116 polymerization reaction Methods 0.000 claims description 2
- 239000007921 spray Substances 0.000 claims description 2
- 229920001897 terpolymer Polymers 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 2
- 125000002496 methyl group Chemical class [H]C([H])([H])* 0.000 claims 2
- RZJRJXONCZWCBN-UHFFFAOYSA-N octadecane Chemical compound CCCCCCCCCCCCCCCCCC RZJRJXONCZWCBN-UHFFFAOYSA-N 0.000 claims 2
- TYFQFVWCELRYAO-UHFFFAOYSA-N suberic acid Chemical compound OC(=O)CCCCCCC(O)=O TYFQFVWCELRYAO-UHFFFAOYSA-N 0.000 claims 2
- WMRCTEPOPAZMMN-UHFFFAOYSA-N 2-undecylpropanedioic acid Chemical compound CCCCCCCCCCCC(C(O)=O)C(O)=O WMRCTEPOPAZMMN-UHFFFAOYSA-N 0.000 claims 1
- 239000004593 Epoxy Substances 0.000 claims 1
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims 1
- 229920000572 Nylon 6/12 Polymers 0.000 claims 1
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 1
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical class C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims 1
- YQGOWXYZDLJBFL-UHFFFAOYSA-N dimethoxysilane Chemical compound CO[SiH2]OC YQGOWXYZDLJBFL-UHFFFAOYSA-N 0.000 claims 1
- 229920001971 elastomer Polymers 0.000 claims 1
- 239000000806 elastomer Substances 0.000 claims 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims 1
- 229920006225 ethylene-methyl acrylate Polymers 0.000 claims 1
- 229920001910 maleic anhydride grafted polyolefin Polymers 0.000 claims 1
- 229940038384 octadecane Drugs 0.000 claims 1
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims 1
- 229920000647 polyepoxide Polymers 0.000 claims 1
- 229920006132 styrene block copolymer Polymers 0.000 claims 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims 1
- 229920002554 vinyl polymer Polymers 0.000 claims 1
- 239000002131 composite material Substances 0.000 abstract description 11
- 238000005034 decoration Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 18
- 238000012360 testing method Methods 0.000 description 18
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 15
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 description 14
- 239000008116 calcium stearate Substances 0.000 description 14
- 235000013539 calcium stearate Nutrition 0.000 description 14
- SDFUXTFVRHBXPH-UHFFFAOYSA-N calcium;octacosanoic acid Chemical compound [Ca].CCCCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O SDFUXTFVRHBXPH-UHFFFAOYSA-N 0.000 description 14
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 description 13
- 229920009204 Methacrylate-butadiene-styrene Polymers 0.000 description 13
- 229920000642 polymer Polymers 0.000 description 13
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- 239000000126 substance Substances 0.000 description 5
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- UHOVQNZJYSORNB-UHFFFAOYSA-N benzene Substances C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 4
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 239000005977 Ethylene Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000007547 defect Effects 0.000 description 3
- 239000002803 fossil fuel Substances 0.000 description 3
- 238000010348 incorporation Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
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- 238000000465 moulding Methods 0.000 description 2
- WLJVNTCWHIRURA-UHFFFAOYSA-N pimelic acid Chemical compound OC(=O)CCCCCC(O)=O WLJVNTCWHIRURA-UHFFFAOYSA-N 0.000 description 2
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- 235000019260 propionic acid Nutrition 0.000 description 2
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 description 2
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- GXURZKWLMYOCDX-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)propane-1,3-diol;dihydroxyphosphanyl dihydrogen phosphite Chemical class OP(O)OP(O)O.OCC(CO)(CO)CO GXURZKWLMYOCDX-UHFFFAOYSA-N 0.000 description 1
- LZHCVNIARUXHAL-UHFFFAOYSA-N 2-tert-butyl-4-ethylphenol Chemical class CCC1=CC=C(O)C(C(C)(C)C)=C1 LZHCVNIARUXHAL-UHFFFAOYSA-N 0.000 description 1
- XOUQAVYLRNOXDO-UHFFFAOYSA-N 2-tert-butyl-5-methylphenol Chemical class CC1=CC=C(C(C)(C)C)C(O)=C1 XOUQAVYLRNOXDO-UHFFFAOYSA-N 0.000 description 1
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- 239000004698 Polyethylene Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
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- TXQVDVNAKHFQPP-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(CO)(CO)CO TXQVDVNAKHFQPP-UHFFFAOYSA-N 0.000 description 1
- MLGZSUJIRZZGNG-UHFFFAOYSA-N [Na].C(CCCCCCCCCCCCCCCCCCCCCCCCCCC)(=O)O Chemical compound [Na].C(CCCCCCCCCCCCCCCCCCCCCCCCCCC)(=O)O MLGZSUJIRZZGNG-UHFFFAOYSA-N 0.000 description 1
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- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 description 1
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- OJDJHGIXNZPZFD-UHFFFAOYSA-N ethyl dihydrogen diphosphate Chemical compound CCO[P@](O)(=O)OP(O)(O)=O OJDJHGIXNZPZFD-UHFFFAOYSA-N 0.000 description 1
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- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical compound CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
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- UTOPWMOLSKOLTQ-UHFFFAOYSA-M octacosanoate Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCC([O-])=O UTOPWMOLSKOLTQ-UHFFFAOYSA-M 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- FATBGEAMYMYZAF-KTKRTIGZSA-N oleamide Chemical compound CCCCCCCC\C=C/CCCCCCCC(N)=O FATBGEAMYMYZAF-KTKRTIGZSA-N 0.000 description 1
- FATBGEAMYMYZAF-UHFFFAOYSA-N oleicacidamide-heptaglycolether Natural products CCCCCCCCC=CCCCCCCCC(N)=O FATBGEAMYMYZAF-UHFFFAOYSA-N 0.000 description 1
- 239000004209 oxidized polyethylene wax Substances 0.000 description 1
- 235000013873 oxidized polyethylene wax Nutrition 0.000 description 1
- 150000008301 phosphite esters Chemical class 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920006124 polyolefin elastomer Polymers 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 125000003003 spiro group Chemical group 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—Polyamides derived from polyamines and polycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses the preparation method of a kind of lightweight reinforced polyamide composition and its composite material, which includes each ingredient of following parts by weight：Polyamide：25 75 parts by weight, modified Hollow Inorganic powder：5 27 parts by weight, alkali-free glass fibre：20 40 parts by weight, bulking agent：1 10 parts by weight；Wherein, polyamide includes polyamide 5X resins.The daiamid composition of the present invention is under the premise of polyamide compoiste material density is reduced, mechanical property, heat resistance for making composite material etc. increases, the promotion of the density and mechanical performance of above-mentioned each ingredient and its content all to lightweight reinforced polyamide plays the role of interwoveness, the lightweight reinforced polyamide resin combination of the present invention, the new performance of polyamide compoiste material is imparted, available for the fields such as automobile instrument panel, building decoration, electric.
Description
Technical field
The present invention relates to a kind of lightweight reinforced polyamide compositions and preparation method thereof.
Background technology
Polyamide refers to the polymer on macromolecular chain with amide groups repetitive unit, with good comprehensive performance,
Such as：High intensity and toughness, high-fire resistance, wearability, chemical resistance, also with self lubricity, self-extinguishment, easy processing etc.
Characteristic is to realize " mould Dai Gang " one of main polymeric material of theory.Since the 1950s, polymer modification is passed through
Method develops a series of Polyamide Engineering Plastic with more excellent properties, and application field is constantly expanded.
Polyamide modified is the hot topic studied now.A kind of new material with property is obtained by modified, is compared
It is a kind of relatively low cost, succinct and direct method for the research and development of new polymers.So-called polymer modification is exactly
Inorganic or organic substance is added in by physics and mechanical means in the polymer or different types of polymer is blended or used
Chemical method realizes the copolymerization of polymer, grafting, block, crosslinking or is combined the above method, makes being manufactured into for material to reach
This decline, moulding processability or end-use properties improved or make polymer material only surface and electricity, magnetic, light,
Heat, sound, burning etc. assign the effect of unique function.
Polymer modification key is " changing ", and it is exactly to bring out one's strengths to make up for one's weaknesses to change, and develops and retains the existing excellent properties of polymer,
The shortcomings that inhibiting and overcoming polymer, and assign polymer new performance according to actual needs.Polymer modification is exactly to polymerize
Seek a best equalization point between the performance of object, processing performance and production cost three.
During being modified to polyamide, it will usually select talcum powder, mica, calcium carbonate, wollastonite, glass fibers
The inorganic material such as dimension, fire retardant carry out blending and modifying, polyamide-based composite material are obtained, to further improve the firm of polyamide
Property, shows glossiness, flammability etc. at heat resistance, dimensional stability, chemical resistance.But the density of inorganic material usually compares
Polyamide it is big, the density for leading to composite material is excessive.
By taking glass fibre as an example, as a kind of inorganic non-metallic material haveing excellent performance, advantage is good insulating, heat-resisting
Property is strong, corrosion resistance is good, high mechanical strength.Glass fibre be typically used as reinforcing material in composite material, electrically insulating material and
Heat-insulating material, Related product are applied to national economy every field.But the density of glass fibre is in 2.4-2.6g/cm3
Between, it is one times of polyamide density or more, after the two is prepared into composite material, density is in 1.2-1.8g/cm3Between,
More than the density of base polyamide polyimide resin, so as to make it is application of the glass fiber-reinforced polyamide composite material in terms of lightweight
It is very limited.
In some application fields, it is desirable to which polyamide compoiste material not only has excellent performance, while it is expected compound
Material has lower density in itself, and such as automotive light weight technology it is expected under the premise of the intensity and security performance for ensureing automobile, to the greatest extent
The kerb weight (weight) of automobile is possibly reduced, so as to improve the dynamic property of automobile, fuel consumption is reduced, it is dirty to reduce exhaust
Dye.It has been proved that car mass reduces half, fuel consumption can also reduce nearly half for experiment.Due to environmental protection and energy-efficient need
Will, the lightweight of automobile has become the trend of world car development.Such as buoy again；The feature density 1.04- of polyamide
1.16 also become limit its key used.
At present, the preparation of lightweight polyamide material is generally realized by foaming technique, such as expanded polystyrene (EPS) (XPS),
Expanded polypropylene (XPP) etc..But in foaming process, shape, size of microvesicle etc. are difficult to control, and usually make polyamide material product
Inside generates defect, loses part excellent performance, and expanded material, often due to stomata is bigger, defect is more, also often makes to gather
The mechanical property for closing object material significantly declines.
Polyamide 5X is a kind of novel high molecular polymer, still the primary stage in research and development, therefore, using it as base
Material prepares lightweight polymeric material, is existing one great challenge of field of macromolecule polymerization.
Invention content
The present invention in order to overcome lightweight polymeric material in the prior art be difficult to meet existing requirement to lightweight, poor performance,
The problem of defect is more provide the preparation method of a kind of novel lightweight reinforced polyamide composition and its composite material.This hair
Bright lightweight reinforced polyamide composition can improve its mechanical property, heat resistance etc., simultaneously while global density is reduced
The processing fluidity of polyamide can be improved.
An object of the present invention：A kind of daiamid composition, the daiamid composition include each of following parts by weight
Ingredient：
Polyamide：25-75 parts by weight,
Modified Hollow Inorganic powder：5-27 parts by weight,
Alkali-free glass fibre：20-40 parts by weight,
With bulking agent：1-10 parts by weight；
Wherein, the polyamide includes polyamide 5X resins.
The preferred technical solution of above-mentioned technical proposal is illustrated below：
A preferred technical solution of the invention, the polyamide 5X refer to 1,5- pentanediamines and dicarboxylic acids for monomer
It polymerize obtained polyamide.Wherein described dicarboxylic acids can be short chain diacid (carbon atom number is less than 10 in carbochain), also may be used
To be long carbochain biatomic acid；Wherein, the short chain diacid preferably includes succinic acid, glutaric acid, adipic acid, pimelic acid, and pungent two
Acid, azelaic acid, preferably decanedioic acid, adipic acid, decanedioic acid；The long carbochain biatomic acid preferably includes eleven carbon diacids, and 12
Carbon dicarboxylic acid, tridecanyldicarboxylic acid, tetradecane diacid, 15 carbon dicarboxylic acids, 16-dicarboxylic acid, seventeen carbon diacids, ten
Eight carbon dicarboxylic acids, maleic acid, Δ 9-1,18 octadecylene binary acid.
A preferred technical solution of the invention, the polyamide can also include its other than polyamide 5X resins
Its polyamide, other described polyamide include：Polyamide 6, polyamide 66, polyamide 69, polyamide 610, polyamide
612nd, it is one or more in polyamide 1010, polyamide 11, polyamide 12 and polyamide 1414.
A preferred technical solution of the invention, it is aggregated that the polyamide 5X includes the monomer of polyamide from biology base
Obtained polyamide；The biological poly amide monomer obtains preferably by biofermentation method or by sustainable day
Right compound is processed through chemical technology to be obtained.It is preferred that the 1,5- pentanediamines is obtain by biofermentation method.
A preferred technical solution of the invention, the polyamide 5X include the biomass source of 35-100%.
A preferred technical solution of the invention, the relative viscosity of 96% (mass percent) sulfuric acid of the polyamide 5X
For 2.4-3.2.
A preferred technical solution of the invention, the polyamide 5X preferred polyamides 56.The polyamide 56 be with 1,
5- pentanediamines and adipic acid are obtained for polymerizable raw material.The relative viscosity of 96% (mass percent) sulfuric acid of the polyamide 56 is excellent
Select 2.4-3.2.
A preferred technical solution of the invention, the modified Hollow Inorganic powder are included with coupling agent to Hollow Inorganic powder
Body is modified the modification Hollow Inorganic powder obtained after processing.The preferred 8-20 weights of parts by weight of the modified Hollow Inorganic powder
Measure part.
Wherein, the coupling agent includes：Silane coupling agent and/or titante coupling agent；
The silane coupling agent preferably includes：Gamma-aminopropyl-triethoxy-silane (NH2CH2CH2CH2Si(OC2H5)3,
Trade name：KH550), g- aminopropyl trimethoxysilanes (NH2(CH2)3Si(OCH3)3, trade name：KH551), γ-(2,3- rings
The third oxygen of oxygen) propyl trimethoxy silicane (CH2-CH(O)CH2-O(CH2)3Si(OCH3)3, trade name：KH560), γ-(methyl-prop
Alkene acyl-oxygen) propyl trimethoxy silicane (CH3CCH2COO(CH2)3Si(OCH3)3, trade name：KH570), N- β-(aminoethyl)-
γ-aminopropyltriethoxy dimethoxysilane (NH2CH2CH2NH2CH2CH2CH2SiCH3(OCH3)2, trade name：KH602)、N-β-
(aminoethyl)-γ-aminopropyltrimethoxysilane (NH2CH2CHNHCH2CH2CH2Si(OCH3)3, trade name：) and ethylene KH792
Ethyl triethoxy silicane alkane (CH2=CHSi (OCH2CH3)3, trade name：KH151 it is one or more in)；
The titante coupling agent preferably includes：Two oleic acid acyloxy of isopropyl (dioctyl phosphoric acid acyloxy) titanate esters
(C55H111O9Ti, trade name：NDZ101), three oleic acid acyloxy of isopropyl (trioctylphosphine phosphoric acid acyloxy) titanate esters
(C54H106O7Ti, trade name：NDZ105), isopropyl three (dioctylphyrophosphoric acid acyloxy) titanate esters (C51H112O22P6Ti, commodity
Name：) and Di(dioctylpyrophosphato) ethylene titanate (C NDZ20134H74O16P4Ti, trade name：NDZ311 one in)
Kind is a variety of.
A preferred technical solution of the invention, the Hollow Inorganic powder include hollow glass micropearl, hollow ceramic powder,
One or more kinds of compositions in hollow titanium dioxide.Preferred 35-70 μm of the grain size of the Hollow Inorganic powder；The sky
The preferred 0.10-0.64g/m of real density of heart inorganic particle3。
A preferred technical solution of the invention, the modified Hollow Inorganic raw powder's production technology include the following steps：
(1) under agitation, it by the solution of the alcohol-water of misty coupling agent, sprays into Hollow Inorganic powder, mixes
It closes, obtains middle product；
(2) middle product is dried, you can.
Wherein, a concentration of 20-40% of the solution of the alcohol-water of the coupling agent, the percentage account for second for coupling agent
The mass percent of alcohol-water solution.
Wherein, the weight ratio of the Hollow Inorganic powder and the coupling agent is (5-25)：(0.01-2).
Wherein, the preferred 600-800rpm of rotating speed during the mixing.
Wherein, preferred 60-80 DEG C of the temperature during mixing.
Wherein, the time of the mixing preferred 3-5min.
Wherein, preferred 70-90 DEG C of the temperature of the drying, more preferable 75-85 DEG C.
Wherein, the time of the drying preferred 8-16h, most preferably more preferable 10-14h, 11-13h.
In the present invention, the alkali-free glass fibre is also known as E glass fibres, refers to the low glass fibers of alkali metal oxide content
Dimension.In general, alkali-free glass fibre R2O content is less than 0.8%, and main component is aluminoborosilicate.
A preferred technical solution of the invention, a diameter of 6-15 μm of the alkali-free glass fibre.
A preferred technical solution of the invention, the bulking agent include：Methyl methacrylate-butadiene-styrene
Copolymer, methyl methacrylate-ethyl acrylate, random ethylene-butyl acrylate copolymer, random ethylene-acrylic acid first
Ester copolymer, random ethylene-methyl acrylate-copolymer-maleic anhydride, Ethylene-butyl acrylate-Glycidyl methacrylate are sweet
Grease copolymer, maleic anhydride grafted polyethylene, maleic anhydride inoculated polypropylene, maleic anhydride stem grafting polyolefin elastomer, horse
Maleic anhydride grafted ethylene propylene diene rubber, maleic anhydride grafted ethene-vinyl acetate, maleic anhydride grafting hydrogenated butadiene-benzene
Ethylene block copolymer, maleic anhydride grafted ethene-butadiene-styrene copolymer, methyl methacrylate-butadiene-benzene
It is one or more in ethylene-dien terpolymer.
A preferred technical solution of the invention, the daiamid composition further include other auxiliary agents, wherein it is described other
Auxiliary agent includes：It is one or more in lubricant, nucleating agent and antioxidant.
A preferred technical solution of the invention, the content of other auxiliary agents is 1-5 parts by weight.
Wherein, the lubricant preferably includes：N, N'- ethylene bis stearamide, oxidized polyethylene wax, polyethylene-acetic acid
Ethylene waxes, partly-hydrolysed polyethylene wax, oleamide, erucyl amide, pentaerythritol stearate, montanate, calcium stearate,
It is one or more in zinc stearate, odium stearate, barium stearate and the macromolecule organic silicon.
Wherein, the nucleating agent preferably includes：P22, montanic acid calcium, montanic acid sodium, polyacrylic acid ionomer, organic illiteracy take off
It is one or more in soil, superfine talcum powder, ultra-fine mica, aluminium oxide and magnesia.
Wherein, antioxidant preferably includes：For N, N- is bis--(3- (3,5- di-tert-butyl-hydroxy phenyls) propiono) oneself two
Amine, β-positive octadecanol ester of (3,5- di-tert-butyl-hydroxy phenyls) propionic acid, three [2.4- di-tert-butyl-phenyls] phosphite esters,
Bis- (2,4- di-tert-butyl-phenyls) propionic acid] pentaerythritol diphosphites, 2,2- methylene-bis- (4- ethyl -6- tert-butyl phenols),
Inclined fourth support-bis--(the 6- tert-butyl-m-cresols) of 4,4-, 1,1,3- tri- (2- methyl -4- hydroxyl -5- tert-butyl-phenyls) butane and 1,3,
It is one or more in 5- trimethyls -2,4,6- three (- 4 hydroxybenzyl of 3,5- di-t-butyls) benzene.
It is a further object to provide a kind of preparation method of polyamide, the preparation method includes following
Step：
By the polyamide, the modified Hollow Inorganic powder, the alkali-free glass fibre and the bulking agent, press
According to ratio as described above, it is uniformly mixed, extrusion molding, you can.
Or, by the polyamide, the modified Hollow Inorganic powder, the alkali-free glass fibre, the bulking agent
With other described auxiliary agents, ratio, is uniformly mixed, extrusion molding as described above, you can.
Wherein, it is preferred that first the polyamide and the bulking agent are uniformly mixed, then with the hollow nothing of the modification
Machine powder and the alkali-free glass fibre are uniformly mixed.
Wherein, it is preferred that the polyamide and the bulking agent are uniformly mixed, and are carried out in mixing machine.
Wherein, it is preferred that when the polyamide and the bulking agent are uniformly mixed, the rotating speed during mixing is
600-800rpm。
Wherein, it is preferred that when the polyamide and the bulking agent are uniformly mixed, the temperature of the mixing is 60-
80℃。
Wherein, it is preferred that the time that the polyamide and the bulking agent are uniformly mixed is 3-5min.
Wherein, it is preferred that the operation being uniformly mixed again with the modified Hollow Inorganic powder and the alkali-free glass fibre,
It carries out in double screw extruder, is more preferably carried out in same phase double screw extruder.
Wherein, it is preferred that the temperature of the double screw extruder is 250-285 DEG C.
Wherein, it is preferred that the rotating speed of the double screw extruder is 150-250rpm, preferably 180-220rpm.
When further including other auxiliary agents in the polyamide, other described auxiliary agents and the polyamide and described
Bulking agent is uniformly mixed, then the operation after carrying out.
Wherein, it is preferred that a kind of preparation method of daiamid composition, the preparation method include the following steps：
(1) polyamide and the bulking agent are uniformly mixed in high-speed mixer, wherein, the high speed is mixed
The rotating speed of conjunction machine is 600-800rpm, incorporation time 3-5min；
(2) main spout of the material through double screw extruder being uniformly mixed in step (1) is added in into double screw extruder
In, and will be added at the modified side spout of the Hollow Inorganic powder through double screw extruder, by alkali-free glass fibre from another
One side spout adds in, and is uniformly mixed, wherein, the temperature of double screw extruder temperature is 250-285 DEG C, and twin-screw rotating speed is
150-250pm。
Wherein, it is to discharge apart from double screw extruder for adding in the side spout of the modified Hollow Inorganic powder
Side spout at die orifice 1/3-3/5 spiro rod lengths position.
Wherein, it is the side spout at nearly discharging die orifice for adding in another side spout of alkali-free glass fibre.
When further including other auxiliary agents in the polyamide, the auxiliary agent is in step (1), with the polyamide resin
Fat and the bulking agent are uniformly mixed.
The present invention prepares lightweight reinforced polyamide using Hollow Inorganic powder and alkali-free glass fibre is modified, wherein, it is modified
Hollow Inorganic powder, alkali-free glass fibre and bulking agent, there is synergistic effect, in the premise for reducing polyamide compoiste material density
Under, mechanical property, heat resistance of composite material etc. is made to increase, above-mentioned each ingredient and its content all enhance polyamides to lightweight
The promotion of the density and mechanical performance of amine plays the role of interwoveness, and lightweight reinforced polyamide composition of the invention is assigned
The performance that polyamide compoiste material is new is given, available for the fields such as automobile instrument panel, building decoration, electric.
On the other hand, the polyamide in the present invention preferably synthesizes to obtain by the monomer of polyamide from biology base.Currently,
For polyamide raw materials more than 99% from fossil fuel, biological poly amide just becomes Showed Very Brisk.The biology of large-scale production
Based polyamide mainly has full biological poly amide and part biological based polyamide, and full biological poly amide is with castor oil, glucose
For raw material, and one kind in the diamine of part biological based polyamide or binary acid starting material is from non-fossil fuel or primary former
Material is from fossil fuel.Compared with traditional polyamide, the industrial chain of biological poly amide is not only reduced to non-renewable resources
Consumption, and GHG emissions mitigation 50% or so.
Specific embodiment
The present invention is described in further detail with reference to embodiments, but the present invention is not limited to these Examples.
The method for testing performance of polyamide is with reference to testing standard once in the present invention：
Density：ISO 1183-1:The non-foam plastic density assay method first part of 2004 plastics：Infusion process, liquid ratio
Weight method and titration；
Tensile property：ISO 527-2:The measure of 1993 plastic tensile performances, second part：Molding and extruding plastics testing
Condition；
Bending property：ISO 178:2001 plastics bending properties are tested；
Izod notched impact strength：ISO 180:The measure of 2001 plastics Chalpy impact performances.
Embodiment 1
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：3597.5g
Alkali-free glass fibre：1000g
Hollow glass micropearl (56 μm of grain size, real density 0.32g/cm3, resistance to compression 13.78MPa)：250g
Bulking agent Methyl Methacrylate-Butadiene-Styrene Copolymer (MBS)：100g
Coupling agent KH-550：2.5g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
The preparation method of 56 resin of lightweight reinforced polyamide：
(1) 50g KH-550 are scattered in 150g alcohol-waters (mass ratio 1：It 1), then under high velocity agitation will mixing in
Solution is uniformly sprayed at the surface of hollow glass micropearl, makes the uniform coated hollow glass bead of coupling agent；High-speed mixer turns
Speed is 600-800rpm, and mixing temperature is 60-80 DEG C, incorporation time 3-5min；
(2) and then by uniformly mixed material 12h is dried under 80 DEG C of environment, obtains modified hollow glass micropearl；
(3) polyamide 56 (PA56), POE-g-MAH, other auxiliary combinations are uniformly mixed in high-speed mixer, at a high speed
The rotating speed of mixing machine be 500-600rpm, mixed at room temperature, incorporation time 3-5min；
(4) the uniformly mixed material that step (3) obtains is positioned in the container of main feeding of extruder；By step
(2) the modification hollow glass micropearl obtained is positioned in the side spout of main feeding side；By alkali-free glass fibre place with
In the side spout of die orifice side；
(5) double screw extruder squeezes out, and each area's (from main feeding section to die head) temperature setting is followed successively by：180℃、220℃、
240 DEG C, 260 DEG C, 270 DEG C, 270 DEG C and 265 DEG C, twin-screw rotating speed is 200rpm；
Wherein, according to this field routine, step (1) and (2), and step (3) can be carried out at the same time, and can also first be carried out
Step (1) and (2) carry out step (2) or, first carry out step (3), then carry out step (1) and (2) again.
The dry 6h at 80 DEG C is sliced by obtained, then prepares test bars, each area's temperature of injection molding machine temperature by iso standard
Degree setting is followed successively by (from spout to nozzle)：240 DEG C, 250 DEG C, 260 DEG C, 265 DEG C and 265 DEG C.Then test bars are existed
48h is sealed at 23 DEG C, is tested according to iso standard.
Test result is referring to table 1.
Embodiment 2
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：2845g
Alkali-free glass fibre：1500g
Hollow glass micropearl (56 μm of grain size, real density 0.32g/cm3, resistance to compression 13.78MPa)：500g
Bulking agent MBS：100g
Coupling agent KH-550：5g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Embodiment 3
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：2092.5g
Alkali-free glass fibre：2000g
Hollow glass micropearl (56 μm of grain size, real density 0.32g/cm3, resistance to compression 13.78MPa)：750g
Bulking agent MBS：100g
Coupling agent KH-550：7.5g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Embodiment 4
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：3097.5g
Alkali-free glass fibre：1500g
Hollow glass micropearl (45 μm of grain size, real density 0.40g/cm3, resistance to compression 27.56MPa)：250g
Bulking agent MBS：100g
Coupling agent KH-550：2.5g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Embodiment 5
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：2345g
Alkali-free glass fibre：2000g
Hollow glass micropearl (45 μm of grain size, real density 0.40g/cm3, resistance to compression 27.56MPa)：500g
Bulking agent MBS：100g
Coupling agent KH-550：5g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Embodiment 6
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：3092.5g
Alkali-free glass fibre：1000g
Hollow glass micropearl (45 μm of grain size, real density 0.40g/cm3, resistance to compression 27.56MPa)：750g
Bulking agent MBS：100g
Coupling agent KH-550：7.5g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Embodiment 7
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：2597.5g
Alkali-free glass fibre：2000g
Hollow glass micropearl (45 μm of grain size, real density 0.46g/cm3, resistance to compression 41.34MPa)：250g
Bulking agent MBS：100g
Coupling agent KH-550：2.5g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Embodiment 8
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：3345g
Alkali-free glass fibre：1000g
Hollow glass micropearl (45 μm of grain size, real density 0.46g/cm3, resistance to compression 41.34MPa)：500g
Bulking agent MBS：100g
Coupling agent KH-550：5g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Embodiment 9
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：2592.5g
Alkali-free glass fibre：1500g
Hollow glass micropearl (45 μm of grain size, real density 0.46g/cm3, resistance to compression 41.34MPa)：750g
Bulking agent MBS：100g
Coupling agent KH-550：7.5g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Embodiment 10
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：1422.5g
Polyamide 1010 (PA1010,96% relative sulfuric acid viscosity 2.66)：1422.5g
Alkali-free glass fibre：1500g
Hollow glass micropearl (56 μm of grain size, real density 0.32g/cm3, resistance to compression 13.78MPa)：500g
Bulking agent MBS：100g
Coupling agent KH-550：5g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Comparative example 1
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：3850g
Alkali-free glass fibre：1000g
Bulking agent MBS：100g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Comparative example 2
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：3350g
Alkali-free glass fibre：1500g
Bulking agent MBS：100g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Comparative example 3
(PA56,2.72) 96% relative sulfuric acid viscosity is to polyamide 56：2850g
Alkali-free glass fibre：2000g
Bulking agent MBS：100g
Other auxiliary combinations (including EBS, calcium stearate, silicone powder, montanic acid calcium, talcum powder, antioxidant 1098)：
50g
Sample preparation and testing procedure are referring to embodiment 1.Dependence test result is referring to table 1.
Table 1：The performance of lightweight reinforced polyamide 5X compositions compares
As seen from the above table：Modified Hollow Inorganic powder, alkali-free glass fibre and bulking agent, under the conditions of specific ratio,
While composite density is reduced, tensile strength, bending strength, bending modulus and the notch punching of composite material can be improved
Hit intensity.
For being modified Hollow Inorganic powder, have one to the properties of lightweight reinforced polyamide resin composite materials
Fixed influence.Also, further, in order to realize better effect, inventor is investigated each of modified Hollow Inorganic powder
Influence of the kind performance parameters to entire light flame-retardant reinforced polyamide resin composite materials, finds：Modified Hollow Inorganic powder
The improvement of real density, compression strength etc. can realize better effect.Such as：The anti-pressure ability pair of modified Hollow Inorganic powder
The influence of weight loss effect is more notable, and modified Hollow Inorganic powder ability is too low, can lead to it in entire lightweight reinforced polyamide
The effect of the loss of weight of resin combination substantially reduces, in other words, under the conditions of on year-on-year basis, the hollow nothing of modification of specific anti-pressure ability
The weight loss effect of machine powder, the effect of the modification Hollow Inorganic powder of significantly larger than general anti-pressure ability.
The above-mentioned description to embodiment be in order to further illustrate with the application of the invention, therefore, the present invention is not limited to implement
Invention content cited by example, those skilled in the art do not depart from the improvement that scope is made according to the announcement of invention
With modification all within protection scope of the present invention.
Claims (12)
1. a kind of daiamid composition, it is characterised in that：The daiamid composition includes each ingredient of following parts by weight：
Polyamide：25-75 parts by weight,
Modified Hollow Inorganic powder：5-27 parts by weight,
Alkali-free glass fibre：20-40 parts by weight,
With bulking agent：1-10 parts by weight；
Wherein, the polyamide includes polyamide 5X resins.
2. daiamid composition as described in claim 1, it is characterised in that：The polyamide 5X refers to 1,5- pentanediamines and two
First carboxylic acid is the polyamide that monomer polymerization obtains；Wherein, the dicarboxylic acids includes：Succinic acid, glutaric acid, adipic acid, heptan two
Acid, suberic acid, azelaic acid, decanedioic acid, eleven carbon diacids, dodecanedicarboxylic acid, tridecanyldicarboxylic acid, tetradecane diacid,
15 carbon dicarboxylic acids, 16-dicarboxylic acid, seventeen carbon diacids, octadecane diacid, maleic acid and Δ 9-1,18 octadecylenes two
It is one or more in first acid.
3. daiamid composition as claimed in claim 2, it is characterised in that：
The polyamide 5X includes the aggregated obtained polyamide of the monomer of polyamide from biology base；
The biological poly amide monomer is preferably obtained by biofermentation method；The polyamide 5X preferably includes 35-100%
Biomass source；
The polyamide 5X preferred polyamides 56；The preferred 2.4-3.2 of relative viscosity of 96% sulfuric acid of the polyamide 56；
And/or the polyamide further includes other polyamides other than polyamide 5X resins, other described polyamide
Including：Polyamide 6, polyamide 66, polyamide 69, polyamide 610, polyamide 612, polyamide 1010, polyamide 11, polyamide
12 and polyamide 1414 in it is one or more.
4. the daiamid composition as described in claim any one of 1-3, it is characterised in that：The modified Hollow Inorganic powder includes
The modification Hollow Inorganic powder obtained after processing is modified Hollow Inorganic powder with coupling agent；
The preferred 8-20 parts by weight of parts by weight of the modified Hollow Inorganic powder.
5. daiamid composition as claimed in claim 4, it is characterised in that：The coupling agent includes：Silane coupling agent and/or
Titante coupling agent；
The silane coupling agent preferably includes：Gamma-aminopropyl-triethoxy-silane, g- aminopropyl trimethoxysilanes, γ-
(the third oxygen of 2,3- epoxies) propyl trimethoxy silicane, γ-(methacryloxypropyl) propyl trimethoxy silicane, N- β-(ammonia second
Base) three second of-γ-aminopropyltriethoxy dimethoxysilane, N- β-(aminoethyl)-γ-aminopropyltrimethoxysilane and vinyl
It is one or more in oxysilane；
The titante coupling agent preferably includes：It is two oleic acid acyloxy of isopropyl (dioctyl phosphoric acid acyloxy) titanate esters, different
Three oleic acid acyloxy of propyl (trioctylphosphine phosphoric acid acyloxy) titanate esters, (dioctylphyrophosphoric acid acyloxy) titanate esters of isopropyl three and
It is one or more in Di(dioctylpyrophosphato) ethylene titanate；
The Hollow Inorganic powder includes one or more in hollow glass micropearl, hollow ceramic powder, hollow titanium dioxide；Institute
State preferred 35-70 μm of the grain size of Hollow Inorganic powder；The preferred 0.10-0.64g/m of real density of the Hollow Inorganic powder3。
6. daiamid composition as claimed in claim 4, it is characterised in that：The modified Hollow Inorganic raw powder's production technology packet
Include following steps：
(1) under agitation, it by the solution of the alcohol-water of misty coupling agent, sprays into Hollow Inorganic powder, mixing obtains
Middle product；
(2) middle product is dried, you can.
7. daiamid composition as claimed in claim 6, it is characterised in that：The concentration of the solution of the alcohol-water of the coupling agent
For 20-40%, the percentage accounts for the mass percent of ethanol-water solution for coupling agent；
And/or the weight ratio of the Hollow Inorganic powder and the coupling agent is (5-25)：(0.01-2)；
And/or the preferred 600-800rpm of rotating speed during the mixing；
And/or preferred 60-80 DEG C of temperature during the mixing；
And/or the time preferred 3-5min of the mixing；
And/or preferred 70-90 DEG C, more preferable 75-85 DEG C of the temperature of the drying；
And/or the time preferred 8-16h, most preferably more preferable 10-14h, 11-13h of the drying.
8. the daiamid composition as described in claim any one of 1-3, it is characterised in that：The alkali-free glass fibre it is a diameter of
6-15μm。
9. the daiamid composition as described in claim any one of 1-3, it is characterised in that：The bulking agent includes：Metering system
Sour methyl esters-butadiene-styrene copolymer, methyl methacrylate-ethyl acrylate, random ethylene-butyl acrylate copolymerization
Object, random ethylene-methyl acrylate copolymer, random ethylene-methyl acrylate-copolymer-maleic anhydride, ethylene-acrylic acid fourth
Ester-glycidyl methacrylate copolymer, maleic anhydride grafted polyethylene, maleic anhydride inoculated polypropylene, maleic anhydride
Grafted polyolefin olefin elastomer, maleic anhydride grafting ethylene propylene diene rubber, maleic anhydride grafted ethene-vinyl acetate, maleic acid
Acid anhydride grafting hydrogenated butadiene-styrene block copolymer, maleic anhydride grafted ethene-butadiene-styrene copolymer, methyl-prop
It is one or more in e pioic acid methyl ester-butadiene-styrene terpolymer.
10. the daiamid composition as described in claim any one of 1-3, it is characterised in that：The daiamid composition further includes
Other auxiliary agents；Other wherein described auxiliary agents include：It is one or more in lubricant, nucleating agent and antioxidant；Described other help
The preferred 1-5 parts by weight of content of agent.
11. a kind of side that polyamide resin composite material is prepared with any one of the claim 1-10 daiamid compositions
Method, it is characterised in that：The preparation method includes the following steps：
By the polyamide, the modified Hollow Inorganic powder, the alkali-free glass fibre and the bulking agent, according to such as
Ratio described in claim 1-10 is uniformly mixed, extrusion molding, you can；
Or, by the polyamide, the modified Hollow Inorganic powder, the alkali-free glass fibre, the bulking agent and institute
Other auxiliary agents are stated, according to the ratio as described in claim 1-10, are uniformly mixed, extrusion molding, you can.
12. preparation method as claimed in claim 11, it is characterised in that：
First the polyamide and the bulking agent are uniformly mixed, then with the modified Hollow Inorganic powder and the alkali-free
Glass fibre is uniformly mixed；
And/or the polyamide and the bulking agent are uniformly mixed, and are carried out in mixing machine；
And/or the rotating speed during mixing is 600-800rpm；
And/or the temperature of the mixing is 60-80 DEG C；
And/or the time that the polyamide and the bulking agent are uniformly mixed is 3-5min；
And/or then be uniformly mixed operation with the modified Hollow Inorganic powder and the alkali-free glass fibre, in twin-screw extrusion
It is carried out in machine；
And/or, it is preferred that the temperature of the double screw extruder is 250-285 DEG C；
And/or, it is preferred that the rotating speed of the double screw extruder is 150-250rpm, more preferably 180-220rpm；
When further including other auxiliary agents in the polyamide, other described auxiliary agents and the polyamide and the increase-volume
Agent is uniformly mixed, then the operation after carrying out.
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| CN111087801A (en) * | 2018-10-24 | 2020-05-01 | 上海凯赛生物技术股份有限公司 | Bio-based polyamide 56 material for heat insulation strip, preparation method and heat insulation strip |
| CN111100454A (en) * | 2019-12-23 | 2020-05-05 | 上海普利特伴泰材料科技有限公司 | Low-dielectric high-strength glass fiber reinforced bio-based PA material and preparation method thereof |
| CN111171565A (en) * | 2019-12-31 | 2020-05-19 | 会通新材料(上海)有限公司 | Polyamide 56 composition with low warpage, high assembly pull force and paint adhesion and application thereof |
| CN111269564A (en) * | 2018-12-04 | 2020-06-12 | 上海凯赛生物技术股份有限公司 | Polyamide 5X abrasive wire and preparation method and application thereof |
| CN111334038A (en) * | 2020-04-26 | 2020-06-26 | 广东中塑新材料有限公司 | PA66 reinforced material and preparation method and application thereof |
| CN111334037A (en) * | 2020-04-23 | 2020-06-26 | 广东中塑新材料有限公司 | PA1010 composite material and preparation method thereof |
| CN111378276A (en) * | 2020-04-29 | 2020-07-07 | 广东中塑新材料有限公司 | PA9T composite material and preparation method thereof |
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| CN111592755A (en) * | 2019-02-21 | 2020-08-28 | 上海凯赛生物技术股份有限公司 | Enhanced bio-based polyamide 56 composition and preparation method thereof |
| CN112159591A (en) * | 2020-10-14 | 2021-01-01 | 上海大赛璐塑料工业有限公司 | Hollow glass bead modified nylon composite material and preparation method and application thereof |
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| CN111269564A (en) * | 2018-12-04 | 2020-06-12 | 上海凯赛生物技术股份有限公司 | Polyamide 5X abrasive wire and preparation method and application thereof |
| CN111592755A (en) * | 2019-02-21 | 2020-08-28 | 上海凯赛生物技术股份有限公司 | Enhanced bio-based polyamide 56 composition and preparation method thereof |
| CN111592755B (en) * | 2019-02-21 | 2022-07-19 | 上海凯赛生物技术股份有限公司 | Enhanced bio-based polyamide 56 composition and preparation method thereof |
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| CN111171565A (en) * | 2019-12-31 | 2020-05-19 | 会通新材料(上海)有限公司 | Polyamide 56 composition with low warpage, high assembly pull force and paint adhesion and application thereof |
| CN111334037A (en) * | 2020-04-23 | 2020-06-26 | 广东中塑新材料有限公司 | PA1010 composite material and preparation method thereof |
| CN111334038A (en) * | 2020-04-26 | 2020-06-26 | 广东中塑新材料有限公司 | PA66 reinforced material and preparation method and application thereof |
| CN111378276A (en) * | 2020-04-29 | 2020-07-07 | 广东中塑新材料有限公司 | PA9T composite material and preparation method thereof |
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| CN111410841B (en) * | 2020-05-06 | 2023-01-03 | 广东中塑新材料有限公司 | PA46 composite material and preparation method thereof |
| CN112159591A (en) * | 2020-10-14 | 2021-01-01 | 上海大赛璐塑料工业有限公司 | Hollow glass bead modified nylon composite material and preparation method and application thereof |
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